Preparation method of vanadium dioxide slurry and preparation method of intelligent temperature control material

By introducing chromium elements into vanadium dioxide slurry to reduce the phase transition temperature and adjusting the light barrier rate through a unique formula, the problems of high phase transition temperature and low infrared light barrier rate in the application of vanadium dioxide in the field of intelligent temperature control are solved, and efficient preparation of intelligent temperature control materials is achieved.

CN120208288APending Publication Date: 2025-06-27CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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Patent Information

Application Number
CN202510522815.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-24
Publication Date
2025-06-27

AI Technical Summary

Technical Problem

The application of vanadium dioxide in the field of intelligent temperature control is limited by its high phase transition temperature. The prior art has shortcomings in reducing the phase transition temperature and it is difficult to effectively adjust the infrared light barrier rate.

Method used

By directly introducing a certain proportion of chromium elements in the preparation process of vanadium dioxide slurry, the phase transition temperature of VO2 is significantly reduced, so that it is lowered to a near room temperature, and the ultraviolet, infrared light barrier rate and solar energy modulation efficiency are regulated through a unique slurry formula.

Benefits of technology

The rapid reduction of VO2 phase transition temperature to near room temperature has been achieved, without affecting other important properties of the material, and the slurry formula significantly improves the light barrier rate and solar energy modulation efficiency, with an effect higher than the market average.

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Abstract

The invention discloses a preparation method of vanadium dioxide slurry and a preparation method of an intelligent temperature control material. The preparation method of the vanadium dioxide slurry comprises the following steps: S1, mixing vanadium leachate and oxalic acid dihydrate according to a preset proportion, and then carrying out hydrothermal reduction reaction; s2, after the reaction is finished, chromium salt is added into the reaction kettle for reaction again, and chromium-doped vanadium dioxide powder is obtained after washing and drying; s3, mixing the vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersing agent and an antioxidant according to a preset proportion, uniformly stirring to obtain slurry, and grinding the slurry. The phase change temperature can be effectively adjusted to be close to the room temperature, the infrared rejection rate can be improved, the steps are simple and easy to operate, the preparation technology is simple, the method is suitable for large-scale production, and the problems that an existing intelligent heat insulation film is not stable enough in performance, short in service life, difficult to industrially produce in a large area and the like are effectively solved.
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Description

Technical Field

[0001] The present invention relates to the technical field of vanadium-based functional materials, and particularly to a preparation method of vanadium dioxide slurry and a preparation method of intelligent temperature control materials. Background Art

[0002] Vanadium dioxide is a metal oxide with phase change properties. Its phase change temperature is 68 °C. The change in structure before and after phase change leads to a reversible transition of infrared light from transmission to reflection. Based on this property, it is applied to the field of preparing intelligent temperature control films. Due to its excellent electrical conductivity, it is also applied to electronic devices.

[0003] However, the relatively high phase change temperature of vanadium dioxide limits its development in practical applications. If it is to be applied to fields such as intelligent temperature control windows, its phase change temperature needs to be adjusted to near room temperature. At the same time, improving the infrared light blocking rate of this material at temperatures above the phase change temperature is the key to the application of this technology.

[0004] Methods for adjusting the phase change temperature include element doping method, stress regulation method, and nanosize effect. Each method has its own advantages and disadvantages. The element doping method adjusts the phase change temperature by introducing other transition metal elements (such as tungsten, molybdenum, chromium, etc.) into the vanadium dioxide lattice; the stress regulation method requires applying external stress to prepare a film to change the lattice structure of VO2 and reduce the phase change temperature, but the process is harsh and large-scale production is not possible; the nanosize effect can reduce the phase change temperature to a certain extent, but the problems of particle agglomeration and slurry stability need to be solved. At the same time, the infrared light blocking rate at temperatures above the phase change temperature is the key to determining the intelligent temperature control effect, and it is also particularly important to adjust the infrared blocking efficiency.

[0005] Therefore, there are still many problems in the application of vanadium dioxide in the field of intelligent temperature control. The existing technology has many deficiencies in reducing the phase change temperature of VO2. There is an urgent need for a simple, effective, and controllable method to rapidly reduce the phase change temperature of VO2 while effectively adjusting the infrared blocking rate.

[0006] In view of this, improvements should be made to the existing technology. Summary of the Invention

[0007] The main object of the present invention is to provide a preparation method of vanadium dioxide slurry and a preparation method of intelligent temperature control materials. By directly introducing a certain proportion of chromium element during the production process, the phase change temperature of VO2 is significantly reduced and can be reduced to near room temperature without affecting other important properties of the material, meeting the actual application requirements; the unique formula of the slurry can greatly regulate the ultraviolet light blocking rate, infrared light blocking rate, and solar modulation efficiency, and the effect is higher than the market average level.

[0008] According to one aspect of the present invention, a method for preparing an intelligent temperature control material is provided, which comprises the following steps: S1. Mix a vanadium leaching solution and oxalic acid dihydrate in a predetermined ratio and then carry out a hydrothermal reduction reaction; S2. After the reaction is completed, add a chromium salt to the reaction kettle for further reaction, and after washing and drying, a chromium-doped vanadium dioxide powder is obtained; S3. Mix the vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersant, and an antioxidant in a predetermined ratio, stir evenly to obtain a slurry, and grind the slurry.

[0009] According to an embodiment of the present invention, the molar ratio of vanadium element in the vanadium leaching solution to oxalic acid dihydrate is 1:(1.5 - 6), the reaction conditions of the hydrothermal reduction reaction are 200 - 400 °C, and the reaction time is 18 - 36 h.

[0010] According to an embodiment of the present invention, the molar ratio of vanadium element in the vanadium leaching solution to chromium element in the chromium salt is (1 - 10):1.

[0011] According to an embodiment of the present invention, the reaction conditions for the further reaction are 150 - 300 °C, and the reaction time is 24 - 48 h; the drying temperature for drying is 30 - 45 °C, and the drying time is 16 - 48 h.

[0012] According to an embodiment of the present invention, the organic solvent includes one or more of ethyl acetate, ethylene glycol, isopropyl alcohol, methyl acetate, and propyl acetate; the light stabilizer includes one or more of o-hydroxybenzophenones, benzotriazoles, salicylate esters, triazines, and substituted acrylonitriles; the infrared light absorber includes one or more of carbon-based materials and ferroelectric materials; the dispersant includes one or more of triethylhexyl phosphate, sodium dodecyl sulfate, methyl pentanol, cellulose derivatives, polyacrylamide, guar gum, and fatty acid polyethylene glycol esters; the antioxidant includes one or more of BHA and BHT.

[0013] According to an embodiment of the present invention, the carbon-based material includes one or more of carbon nanotubes, graphene, and nano carbon black; the ferroelectric material includes one or more of iron tetroxide and strontium titanate.

[0014] According to an embodiment of the present invention, the mass ratio of the vanadium dioxide powder to the organic solvent, the dispersant, the antioxidant, the light stabilizer, and the infrared light absorber is (9 - 12):(18 - 30):(4 - 6):(3.5 - 4.5):(0.8 - 1.2):(0.8 - 1.2).

[0015] According to an embodiment of the present invention, the vanadium concentration of the vanadium leaching solution is 30 - 60 g / L; and / or the chromium salt includes chromium sulfate; and / or in step S3, grinding is performed until the particle size in the slurry is in the range of 30 - 150 nm.

[0016] According to another aspect of the present invention, a method for preparing an intelligent temperature control material is provided, including: mixing a vanadium dioxide slurry with a film-forming agent or a coating in a predetermined ratio, wherein the vanadium dioxide slurry is prepared by the method of any one of the above technical solutions.

[0017] According to an embodiment of the present invention, the mass ratio of the slurry to the film-forming agent or the coating is 1:(10 - 40).

[0018] In the method for preparing a vanadium dioxide slurry according to an embodiment of the present invention, by directly introducing a certain proportion of chromium element during the production process, the phase transition temperature of VO2 is significantly reduced, and it can be reduced to near room temperature without affecting other important properties of the material, meeting the actual application requirements; the unique formula of the slurry can greatly regulate the ultraviolet light blocking rate, infrared light blocking rate, and solar modulation efficiency, and the effect is higher than the market average level. Description of the Drawings

[0019] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0020] Figure 1 The process flow diagram of a method for preparing a vanadium dioxide slurry according to an exemplary embodiment of the present invention is shown. Detailed Embodiments

[0021] The following detailed description of the embodiments is used to exemplarily illustrate the principle of the present invention, but cannot be used to limit the scope of the present invention. The present invention can be implemented in many different forms, not limited to the specific embodiments disclosed herein, but including all technical solutions falling within the scope of the claims.

[0022] The present invention provides these embodiments to make the present disclosure thorough and complete, and to fully convey the scope of the present invention to those skilled in the art. It should be noted that: unless otherwise specifically stated, the relative arrangements of the components and steps, the components of the materials, the numerical expressions and values described in these embodiments should be construed as merely exemplary, rather than as limitations.

[0023] It should be noted that in the description of the present invention, unless otherwise specified, the meaning of "a plurality" is greater than or equal to two; the orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "inner", "outer", etc. is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present invention. When the absolute position of the described object changes, the relative position relationship may also change accordingly.

[0024] It should also be noted that in the description of the present invention, unless otherwise clearly defined and limited, the terms "mounted", "connected", and "coupled" should be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or an integral connection; it may be directly connected, or indirectly connected through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. When it is described that a specific device is located between a first device and a second device, there may or may not be an intermediate device between the specific device and the first device or the second device.

[0025] All terms used in the present invention have the same meanings as those understood by ordinary skilled artisans in the field to which the present disclosure pertains, unless otherwise specifically defined. It should also be understood that terms defined in a general dictionary, such as those, should be interpreted as having meanings consistent with their meanings in the context of the relevant art, and should not be interpreted in an idealized or overly formal sense, unless specifically defined as such here.

[0026] Technologies, methods, and devices known to those of ordinary skill in the relevant fields may not be discussed in detail, but where appropriate, these technologies, methods, and devices should be regarded as part of the specification.

[0027] As Figure 1 shown, the present invention provides a method for preparing an intelligent temperature control material, which includes the following steps: S1. Mix the vanadium leaching solution and oxalic acid dihydrate in a predetermined ratio and then carry out a hydrothermal reduction reaction; S2. After the reaction is completed, add a chromium salt to the reaction kettle for further reaction, and after washing and drying, obtain chromium-doped vanadium dioxide powder; S3. Mix the vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersant, and an antioxidant in a predetermined ratio, stir evenly to obtain a slurry, and grind the slurry.

[0028] In the intelligent temperature control material and its preparation method according to the embodiments of the present invention, by directly introducing a certain proportion of chromium elements during the production process, the phase transition temperature of VO2 is significantly reduced and can be reduced to near room temperature without affecting other important properties of the material, meeting the actual application requirements; the unique formula of the slurry can greatly regulate the ultraviolet light blocking rate, infrared light blocking rate and solar modulation efficiency, and the effect is higher than the market average level.

[0029] In some specific embodiments, the molar ratio of vanadium element in the vanadium leaching solution to oxalic acid dihydrate is 1:(1.5 - 6), and the reaction conditions for the hydrothermal reduction reaction are 200 - 400 °C and the reaction time is 18 - 36 h. The hydrothermal reaction utilizes the reducibility of oxalate ions to reduce vanadium in the solution from +5 valence to +4 valence to form vanadyl oxalate. By controlling the reaction temperature, time and doping amount, the oxidation state of vanadium can be precisely adjusted, thereby affecting the critical phase transition temperature of the final product VO2.

[0030] Based on the above embodiments, the molar ratio of vanadium element in the vanadium leaching solution to chromium element in the chromium salt is (1 - 10):1. The vanadium leaching solution is a sulfuric acid system, and the chromium salt can be chromium sulfate. After adding, the reaction continues.

[0031] In some specific embodiments, the reaction conditions for the re-reaction are 150 - 300 °C and the reaction time is 24 - 48 h; the drying temperature for drying is 30 - 45 °C and the drying time is 16 - 48 h. At this time, vanadium dioxide powder with a modulated phase transition temperature is obtained.

[0032] Based on the above embodiments, the organic solvent includes one or more of ethyl acetate, ethylene glycol, isopropyl alcohol, methyl acetate and propyl acetate. When the organic solvent is a mixture of two reagents, the mixing mass ratio is (1 - 5):1.

[0033] The light stabilizer includes one or more of o-hydroxybenzophenones, benzotriazoles, salicylate esters, triazines, substituted acrylonitriles. The light stabilizer can effectively absorb ultraviolet light with a wavelength of 290 - 410 nm and rarely absorb visible light. It has good thermal stability and light stability itself, and can prevent or delay the process of photoaging, so as to achieve the purpose of extending the service life of polymer products.

[0034] The infrared light absorber includes one or more of carbon-based materials and ferroelectric materials. The carbon-based materials include one or more of carbon nanotubes, graphene and nano carbon black. The carbon-based materials have good infrared absorption performance and optical properties; the ferroelectric materials include one or more of iron tetroxide and strontium titanate. The ferroelectric materials have good infrared absorption performance and thermal response performance.

[0035] The dispersant includes one or more of triethylhexyl phosphate, sodium dodecyl sulfate, methyl pentanol, cellulose derivatives, polyacrylamide, guar gum, and fatty acid polyethylene glycol ester. By reducing the surface tension, the dispersant evenly disperses the solid particles in the temperature control material in the resin or matrix, avoiding agglomeration.

[0036] The antioxidant includes one or more of BHA and BHT. The antioxidant works in coordination with the dispersant to keep the performance of the temperature control material stable in the range of -20~80°C. Based on the above embodiments, the mass ratio of vanadium dioxide powder to the organic solvent, dispersant, antioxidant, light stabilizer, and infrared light absorber is (9~12):(18~30):(4~6):(3.5~4.5):(0.8~1.2):(0.8~1.2), for example, it can be (9~12):(18~30):(4~6):4:1:1.

[0037] In some specific embodiments, the vanadium concentration of the vanadium leaching solution is 30~60 g / L; and / or the chromium salt includes chromium sulfate; and / or in step S3, it is ground until the particle size of the particles in the slurry is in the range of 30~150 nm. Particles with a particle size of 30~150 nm can be more evenly dispersed in the slurry, ensuring the synchronism of the phase change process and the sudden change characteristics of the conductivity, so that when used as a photoelectric switch material, it has higher sensitivity and stability.

[0038] The present invention also proposes a preparation method of an intelligent temperature control material, which includes: mixing the vanadium dioxide slurry with a film-forming agent or coating according to a predetermined ratio, wherein the vanadium dioxide slurry is prepared by the method of any one of the above technical solutions.

[0039] In some specific embodiments, mixing the vanadium dioxide slurry with a film-forming agent or coating according to a predetermined ratio specifically includes mixing the slurry with polyurethane varnish and then using the coating method to load it onto a transparent PET film for performance testing.

[0040] For the convenience of reflecting the excellent performance of the slurry and the rapid simplicity of the front-end preparation process, the present invention mixes this slurry with polyurethane varnish and uses the coating method to load it onto a transparent PET film for performance testing.

[0041] Based on the above embodiments, the mass ratio of the slurry to the film-forming agent or coating is 1:(10~40).

[0042] Mix the prepared slurry with the materials required for later applications according to a ratio of 1:(10~40) and continue with the subsequent applications. For example, when used as intelligent temperature control glass later, it is mixed with a film-forming agent to form a film and then made into laminated glass; or when used as a coating material, the slurry is simply mixed with the coating.

[0043] The present application will be described below with specific embodiments.

[0044] Example 1: Step 1: Mix a vanadium leaching solution with a vanadium concentration of 50 g / L and oxalic acid dihydrate for hydrothermal reduction, where the molar ratio of vanadium to oxalic acid dihydrate is 1:2, and the hydrothermal conditions are a temperature of 280 °C and a reaction time of 18 h.

[0045] Step 2: After the above reaction is completed, add chromium sulfate to the reaction kettle. The molar ratio of vanadium to chromium is 5:1, and the reaction continues at a temperature of 200 °C for a reaction time of 24 h. After washing and drying, chromium-doped vanadium dioxide is obtained. The drying temperature is 30 °C and the drying time is 30 h. At this time, vanadium dioxide powder with a modulated phase transition temperature is obtained. The phase transition temperature of the powder is measured to be 31.2 °C using DSC (Differential Scanning Calorimetry).

[0046] Step 3: Mix the modulated vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersant, and an antioxidant, and stir evenly, and then grind in a sand mill until the particle size in the slurry is within 100 nm to stop grinding. The organic solvent is ethyl acetate, the light stabilizer is o-hydroxybenzophenone, the infrared light absorber is nano-carbon black (50 nm), the dispersant is sodium dodecyl sulfate, and the antioxidant is BHA (butylated hydroxyanisole). Among them, the mass ratio of vanadium dioxide powder to the organic solvent, the dispersant, the antioxidant, the light stabilizer, and the infrared light absorber is 9:18:4:4:1:1.

[0047] Step 4: Mix the prepared slurry with polyurethane varnish in a mass ratio of 1:10 and stir evenly, and then perform performance testing on a transparent PET film by the coating method. The coating thickness is 50 μm. The low-temperature visible light transmittance is 74.2%, the high-temperature visible light transmittance is 70.6%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 78.2%, and the solar light adjustment efficiency is 16.2%. After high-temperature and high-humidity aging for 240 h, the low-temperature visible light transmittance is 77%, the high-temperature visible light transmittance is 72%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 75.4%, and the solar light adjustment efficiency is 15.6%.

[0048] Example 2: Step 1: Mix a vanadium leaching solution with a vanadium concentration of 45 g / L and oxalic acid dihydrate for hydrothermal reduction, where the molar ratio of vanadium to oxalic acid dihydrate is 1:3, and the hydrothermal conditions are a temperature of 320 °C and a reaction time of 24 h.

[0049] Step 2: After the above reaction is completed, add chromium sulfate to the reaction kettle. The molar ratio of vanadium to chromium is 10:1, and the reaction continues at a temperature of 150 °C for 36 h. After washing and drying, vanadium-doped vanadium dioxide is obtained. The drying temperature is 35 °C and the drying time is 36 h. At this time, vanadium dioxide powder with a modulated phase transition temperature is obtained.

[0050] Step 3: Then mix the modulated vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersant, and an antioxidant, stir evenly, and grind in a sand mill until the particle size in the slurry reaches 50 nm to stop grinding. The organic solvent is a mixture of ethyl acetate and ethylene glycol, and the mixing mass ratio is 5:1. The light stabilizer is selected as salicylate, the infrared light absorber is selected as single-walled carbon nanotubes, the dispersant is guar gum, and the antioxidant is BHT (dibutylhydroxytoluene). Among them, the mass ratio of vanadium dioxide powder to the organic solvent, the dispersant, the antioxidant, the light stabilizer, and the infrared light absorber is 10:30:5:4:1:1.

[0051] Step 4: Mix the prepared slurry with polyurethane varnish evenly according to a mass ratio of 1:20, and perform performance testing on a transparent PET film by the coating method. The coating thickness is 50 μm. The low-temperature visible light transmittance is 75.1%, the high-temperature visible light transmittance is 71.4%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 79.1%, and the solar light adjustment efficiency is 15.9%. After high-temperature and high-humidity aging for 240 h, the low-temperature visible light transmittance is 76.2%, the high-temperature visible light transmittance is 73.3%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 76.1%, and the solar light adjustment efficiency is 15.1%.

[0052] Example 3: Step 1: Hydrothermally reduce a vanadium leaching solution with a vanadium concentration of 35 g / L and dihydrate oxalic acid. The molar ratio of vanadium to dihydrate oxalic acid is 1:5, and the hydrothermal conditions are a temperature of 220 °C and a reaction time of 24 h.

[0053] Step 2: After the reaction is completed, add chromium sulfate to the reaction kettle. The molar ratio of vanadium to chromium is 8:1, and the reaction continues at a temperature of 200 °C for 24 h. After washing and drying, vanadium-doped vanadium dioxide is obtained. The drying temperature is 35 °C and the drying time is 32 h. At this time, vanadium dioxide powder with a modulated phase transition temperature is obtained.

[0054] Step 3: Then, mix the modulated vanadium dioxide powder with organic solvents, light stabilizers, infrared light absorbers, dispersants, and antioxidants, stir evenly, and grind in a sand mill until the particle size in the slurry reaches 150 nm to stop grinding. The organic solvent is a mixture of ethyl acetate and isopropanol with a mixing mass ratio of 4:1. The light stabilizer is benzotriazole, the infrared light absorber is strontium titanate, the dispersant is methyl pentanol, and the antioxidant is BHA (butylated hydroxyanisole). Among them, the mass ratio of vanadium dioxide powder to organic solvent, dispersant, antioxidant, light stabilizer, and infrared light absorber is 9:27:6:4:1:1.

[0055] Step 4: After mixing the prepared slurry and polyurethane varnish evenly according to a mass ratio of 1:15, perform performance testing on a transparent PET film by the coating method. The coating thickness is 50 μm. The low-temperature visible light transmittance is 74.6%, the high-temperature visible light transmittance is 69.2%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 78.6%, and the solar modulation efficiency is 16.7%. After 240 h of high-temperature and high-humidity aging, the low-temperature visible light transmittance is 76.7%, the high-temperature visible light transmittance is 72.1%, the ultraviolet light barrier rate is 100%, the infrared light barrier rate is 75.6%, and the solar modulation efficiency is 15.9%.

[0056] After the implementation of the present invention, it has at least the following beneficial effects: (1) Rapidly reduce the phase transition temperature: By directly introducing a certain proportion of chromium elements during the production process, the phase transition temperature of VO2 is significantly reduced and can be reduced to near room temperature without affecting other important properties of the material, meeting the actual application requirements.

[0057] (2) The unique formula of the slurry can greatly regulate the ultraviolet light barrier rate, infrared light barrier rate, and solar modulation efficiency, and the effect is higher than the market average level.

[0058] (3) The preparation method has a simple process, a wide range of application scenarios without restricting the substrate, is green and environmentally friendly throughout the process, and is suitable for large-scale production.

[0059] (4) It has a wide range of applications, especially in the fields of new energy vehicles, building glass, aerospace, building facades, and electromagnetic waves.

[0060] The above are the exemplary embodiments disclosed by the present invention. The order of disclosure of the above embodiments of the present invention is only for description and does not represent the superiority or inferiority of the embodiments. However, it should be noted that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of disclosure of the embodiments of the present invention (including the claims) is limited to these examples. Without departing from the scope defined by the claims, various changes and modifications can be made. The functions, steps, and / or actions of the method claims according to the disclosed embodiments here do not need to be executed in any specific order. In addition, although the elements disclosed in the embodiments of the present invention can be described or claimed in an individual form, they can also be understood as plural unless explicitly limited to the singular form.

[0061] Those of ordinary skill in the art should understand that: the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of disclosure of the embodiments of the present invention (including the claims) is limited to these examples; under the concept of the embodiments of the present invention, the technical features between the above embodiments or different embodiments can also be combined, and there are many other variations in different aspects of the embodiments of the present invention as described above, and they are not provided in detail for the sake of brevity. Therefore, any omission, modification, equivalent replacement, improvement, etc. made within the spirit and principle of the embodiments of the present invention shall be included within the protection scope of the embodiments of the present invention.

Claims

1. A method for preparing vanadium dioxide slurry, characterized in that: The following steps are involved: S1, mixing the vanadium leaching solution and oxalic acid dihydrate in a predetermined ratio and then performing a hydrothermal reduction reaction; S2. After the reaction is completed, chromium salt is added to the reactor for further reaction, and chromium-doped vanadium dioxide powder is obtained after washing and drying; S3, mixing the vanadium dioxide powder with an organic solvent, a light stabilizer, an infrared light absorber, a dispersant and an antioxidant in a predetermined ratio, stirring the mixture evenly to obtain a slurry, and grinding the slurry.

2. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The molar ratio of the vanadium element in the vanadium leaching solution to the dihydrated oxalic acid is 1:(1.5-6), the reaction conditions of the hydrothermal reduction reaction are 200-400° C., and the reaction time is 18-36 hours.

3. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The molar ratio of the vanadium element in the vanadium leaching solution to the chromium element in the chromium salt is (1-10):

1.

4. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The reaction conditions of the re-reaction are 150-300° C. and the reaction time is 24-48 hours; the drying temperature of the drying is 30-45° C. and the drying time is 16-48 hours.

5. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The organic solvent includes one or more of ethyl acetate, ethylene glycol, isopropanol, methyl acetate and propyl acetate; the light stabilizer includes one or more of o-hydroxybenzophenone, benzotriazole, salicylate, triazine and substituted acrylonitrile; the infrared light absorber includes one or more of carbon-based materials and ferroelectric materials; the dispersant includes one or more of triethylhexyl phosphate, sodium dodecyl sulfate, methyl amyl alcohol, cellulose derivatives, polyacrylamide, guar gum and fatty acid polyethylene glycol esters; the antioxidant includes one or more of BHA and BHT.

6. The method for preparing vanadium dioxide slurry according to claim 5, characterized in that: The carbon-based material includes one or more of carbon nanotubes, graphene and nano carbon black; the ferroelectric material includes one or more of ferroferric oxide and strontium titanate.

7. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The mass ratio of the vanadium dioxide powder to the organic solvent, dispersant, antioxidant, light stabilizer and infrared light absorber is (9-12): (18-30): (4-6): (3.5-4.5): (0.8-1.2): (0.8-1.2).

8. The method for preparing vanadium dioxide slurry according to claim 1, characterized in that: The vanadium concentration of the vanadium leaching solution is 30-60 g / L; and / or the chromium salt includes chromium sulfate; and / or in step S3, the particles in the slurry are ground to a particle size in the range of 30-150 nm.

9. A method for preparing an intelligent temperature control material, characterized in that: include: The vanadium dioxide slurry is mixed with a film-forming agent or a coating in a predetermined ratio, wherein the vanadium dioxide slurry is prepared by the method described in any one of claims 1 to 8 above.

10. The method for preparing the intelligent temperature control material according to claim 9, characterized in that: The mass ratio of the slurry to the film-forming agent or coating is 1: (10-40).